The MSr2Y1.5Ce0.5Cu2Oz (M-1222) compounds, with M = Fe and Co, have been synthesized through a solid-state reaction route. Both compounds crystallize in a tetragonal structure (space group 14/mmm). A Rietveld structural refinement of the room-temperature neutron diffraction data for Fe-1222 reveals that nearly half the Fe remains at the M site, while the other half goes to the Cu site in the CuO2 planes. Existence of Fe at two different lattice sites is also confirmed by 57Fe Mössbauer spectroscopy from which it is inferred that ~50% of the total Fe occupies the Cu site in the CuO2 planes as Fe3+, whereas the other ~50% is located at the M site with ~40% as Fe4+ and ~10% as Fe3+. For the M[Double Bond]Co compound, nearly 84% of Co remains at its designated M site, while the rest occupies the Cu site in the CuO2 planes